原料预处理对BaTiO3压电陶瓷的物性影响

doi:10.15541/jim20160489

摘要/Abstract

摘要：

BaCO₃微粉原料通常由尺寸较大的棒状颗粒所组成, 这些棒状颗粒在一次球磨过程中由于不容易粉碎, 从而对经预烧、二次球磨所得到的BaTiO₃陶瓷微粉的化学组分的均匀性和颗粒度产生影响, 进而影响后序烧结制备的BaTiO₃陶瓷的微观组织结构和压电性能。本研究重点探讨了以BaCO₃和TiO₂为原料、通过固相反应途径制备BaTiO₃陶瓷时, 实施原料预处理对所制备的BaTiO₃压电陶瓷物性的影响。研究发现, 配料前对BaCO₃原料实施球磨预处理可明显地降低棒状颗粒的尺寸, 从而可获得颗粒度细化的BaTiO₃陶瓷微粉, 进而制备致密度更高和晶粒尺寸更小而压电性能更高的BaTiO₃陶瓷材料。研究中对BaCO₃微粉进行不同时间的球磨预处理, 然后制备钛酸钡陶瓷, 考察了其压电性能、介电性质、铁电性能和微观结构等物理性质。利用同样的BaCO₃微粉原料, 未经球磨预处理所制备的BaTiO₃陶瓷的压电系数d₃₃最高值为410 pC/N, 而实施合适的球磨预处理制备的BaTiO₃陶瓷的压电系数d₃₃最高值可达470 pC/N。

关键词: BaTiO₃, 压电陶瓷, 原料预球磨处理, 微观结构

Abstract:

BaCO₃ powder usually consists of large rod-shaped particles, which can not be easily broken up into fine ones when ball-milled together with TiO₂ powder. This may lead to chemical compositional non-uniformity and large particle sizes of the subsequently synthesized BaTiO₃ powder through the calcination and the secondary ball-milling procedure, and may eventually affect the microstructure and the piezoelectric properties of resultant BaTiO₃ ceramics. Effects of the pre-milling treatment of BaCO₃powder on physical properties of the resultant BaTiO₃ ceramics prepared by conventional solid-state reaction were investigated. The results show that an additional ball-milling treatment of BaCO₃ powder before being mixed with TiO₂ powder can remarkably reduce the size of the rod-like particles, which is an effective way to get good-quality BaTiO₃fine powder. In such a way, a series of small-grained dense BaTiO₃ ceramics are fabricated with significantly high piezoelectric coefficient d₃₃. The BaTiO₃ceramics were prepared with the BaCO₃ powders ball-milled for different time before mixing with raw TiO₂ powder. Physical properties of the resultant BaTiO₃ceramics, including piezoelectric properties, dielectric properties, ferroelectric properties, and microstructure were investigated. A much enhanced d₃₃value of 470 pC/N was achieved for the BaTiO₃ ceramics prepared with the BaCO₃ powders ball-milled for 8 h, in comparison to the maximum value of 410 pC/N for those BaTiO₃ ceramics prepared with un-ball-milled BaCO₃ powders.

Key words: BaTiO₃, piezoelectric ceramics, pre-milling of raw material, microstructure

中图分类号:

TQ174

孙丹丹, 张家良, 武燕庆, 张仲秋, 刘大康. 原料预处理对BaTiO₃压电陶瓷的物性影响[J]. 无机材料学报, 2017, 32(6): 615-620.

SUN Dan-Dan, ZHANG Jia-Liang, WU Yan-Qing, ZHANG Zhong-Qiu, LIU Da-Kang. Raw-material Pre-milling on Physical Property of BaTiO₃ Piezoelectric Ceramics[J]. Journal of Inorganic Materials, 2017, 32(6): 615-620.

图/表 8

图1 BaCO3微粉的微观形貌

Fig. 1 SEM images of BaCO3 powders(a) Raw material of BaCO3 powders; (b)-(e) Ball-milling BaCO3 powders for 4, 6, 8, and 10 h, respectively

图2 BaTiO3陶瓷微粉的微观形貌

Fig. 2 SEM images of BaTiO3 ceramic powders(a) Prepared with untreated BaCO3 powders; (b)-(e) Prepared with ball-milling BaCO3 powders for 4, 6, 8, and 10 h, respectively

表1 不同预球磨处理条件的BaCO3微粉为原料所制备的BaTiO3陶瓷的诸种物理性质

Table 1 Physical properties of BaTiO3 ceramics prepared with ball-milling BaCO3 powders for different time

Premilling time/h	Sinter. temp. /℃	ρ/%	g/μm	d₃₃/(pC·N^-1)	ε’ at 1 kHz	tanδ/%	T_O-T/℃	T_C/℃
0	1210	95.6	3.4	370	3212	3.1	-	-
0	1220	97.8	3.5	410	3370	3.1	27.8	121.8
4	1230	96.5	1.3	450	3547	3.1	25.6	121.5
6	1230	96.9	1.9	440	3350	2.9	27.2	122.6
8	1230	96.1	1.4	470	4133	2.9	28.2	120.6
10	1230	95.7	1.4	465	3560	3.1	25.8	122.1

图3 不同预球磨处理条件的BaCO3微粉为原料所制备的BaTiO3陶瓷的介电温谱

Fig. 3 Temperature dependence of dielectric permittivity for the various BaTiO3 ceramic prepared with ball-milling BaCO3 powders for different time

图4 不同预球磨条件制备的BaTiO3陶瓷的微观结构

Fig. 4 SEM images of microstructure for various BaTiO3 ceramics prepared with ball-milling BaCO3 powders for different time(a) Prepared with untreated BaCO3 powder; (b)-(e) Prepared with ball-milling BaCO3 powders for 4, 6, 8, and 10 h, respectively

图5 不同预球磨处理条件的BaCO3微粉为原料所制备的BaTiO3陶瓷微粉的XRD图谱

Fig. 5 XRD patterns of the various BaTiO3 ceramic powders prepared with ball-milling BaCO3 powders for different time

图6 室温下测得的各种BaTiO3陶瓷的P-E电滞回线

Fig. 6 Curves of P-E loops for the various BaTiO3 ceramics measured at room temperature

图7 不同的预球磨时间制备的BaTiO3陶瓷的剩余极化强度和矫顽场的变化

Fig. 7 Variations of Pr and Ec of BaTiO3 ceramics obtained with different ball-milling time of BaCO3 powders

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原料预处理对BaTiO₃压电陶瓷的物性影响

Raw-material Pre-milling on Physical Property of BaTiO₃ Piezoelectric Ceramics

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